Methods for electrically forming materials; and mixed metal materials

ABSTRACT

The invention includes a method of forming a material which comprises at least two elements. More specifically, the method comprises providing an electrolytic cell comprising a cathode, an anode, and an electrolytic solution extending between the cathode and anode. A metallic product is electrolytically formed within the electrolytic cell. The forming of the metallic product comprises primarily electrorefining of a first element of the at least two elements and primarily electrowinning of a second element of the at least two elements. The invention also includes a mixed metal product comprising at least two elements, such as a product comprising tantalum and titanium.

TECHNICAL FIELD

[0001] The invention pertains to methods of electrically formingmaterials comprising at least two elements, and in particularapplications pertains to methods of forming materials comprisingtantalum and titanium. The invention also pertains to mixed metalmaterials, such as materials comprising tantalum and titanium. Inaddition, the invention pertains to sputtering targets made of mixedmetal materials, such as targets comprising tantalum and titanium.

BACKGROUND OF THE INVENTION

[0002] Numerous applications exist in which it can be desired to formmaterials comprising two or more elements provided in a substantiallyhomogenous distribution of the elements. For instance, it can be desiredto form physical vapor deposition (PVD) targets comprising two or moremetallic elements uniformly distributed throughout the targets.Frequently, it is difficult to combine two or more elements into ahomogenous mixture when their melting points and/or densities are farapart. For example, there could be an interest to develop an alloyedtitanium-tantalum target. However, making an alloyed titanium-tantalumingot is impractical with conventional techniques. A large differencebetween the melting points of titanium and tantalum (1670° C. fortitanium and 2996° C. for tantalum) makes it impractical to melttitanium together with tantalum in an e-beam furnace. Titanium would besimply vaporized at the melting point of tantalum. In addition, thelarge difference in densities (4.5 g/cm³ for titanium and 16 g/cm³ fortantalum) would be troublesome when powder processing an alloycomprising both titanium and tantalum. Segregation could too easily takeplace. Additionally, because of a generally higher gas content, powderprocessed targets are less preferred than melted and wrought targets.

[0003] It would be desirable to develop new methods for forming mixedmetal alloy ingots, and it would be particularly desirable to developmethods which could be utilized to form titanium and tantalum alloyingots. More generally, it would be desirable to develop new methods forforming products comprising mixtures of two or more elements. It isknown that if an alloyed feedstock is melted, the melting point of thefeedstock is between the melting points of components. Specifically, ifan alloyed titanium and tantalum piece were melted, it would melt at atemperature in between the melting points of titanium and tantalum. Thehigher the portion of titanium in the piece, the lower would be themelting temperature. The lowering of the melting temperature could makethe melting process much easier than for a material comprising puretantalum. Therefore, it could be desirable to develop new methods forpreparing tantalum materials diluted with titanium to form alloyedtantalum feedstocks for melting processes.

SUMMARY OF THE INVENTION

[0004] In one aspect, the invention encompasses a method of forming amaterial which comprises at least two elements. More specifically, themethod comprises providing an electrolytic cell comprising a cathode, ananode, and an electrolytic solution extending between the cathode andanode. A metallic product is electrolytically formed within theelectrolytic cell. The forming of the metallic product comprisesprimarily electrorefining of a first element of the at least twoelements and primarily electrowinning of a second element of the atleast two elements.

[0005] In another aspect, the invention encompasses a method forelectrolytically forming a material, wherein an electrolytic cell isprovided which comprises a cathode, at least two anodes, and anelectrolytic solution extending between the cathode and the at least twoanodes. The at least two anodes comprise first and second anodes havingdifferent concentrations of a first element relative to another. Theelectrolytic solution comprises a compound which includes a secondelement. A metallic product is electrolytically formed with theelectrolytic cell. The metallic product comprises a mixture of the firstand second elements.

[0006] In yet another aspect, the invention encompasses a method forelectrolytically forming a product which comprises a mixture of tantalumand titanium.

[0007] In yet another aspect, the invention encompasses a mixed metalproduct comprising at least two elements, such as a product comprisingtantalum and titanium. The product comprising a mixture of the at leasttwo elements can be considered an alloyed product, and can be used asfeedstock for melting processes. In particular, a product comprisingtitanium and tantalum can be melted in an e-beam furnace to form atitanium-tantalum alloy ingot for further processing into a sputteringtarget.

BRIEF DESCRIPTION OF THE DRAWINGS

[0008] Preferred embodiments of the invention are described below withreference to the following accompanying drawings.

[0009]FIG. 1 is a diagrammatic, cross-sectional view of an apparatuswhich can be utilized for methodology of the present invention.

[0010]FIG. 2 is a diagrammatic, cross-sectional view of a secondapparatus which can be utilized for methodology of the presentinvention.

[0011]FIG. 3 is a diagrammatic, cross-sectional view of a sputteringtarget/backing plate structure which can be formed in accordance withmethodology of the present invention.

[0012]FIG. 4 is a diagrammatic top view of the structure of FIG. 3, withthe cross-sectional view of FIG. 3 indicated by the line 3-3 of thefigure.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0013] In one aspect, the invention encompasses a method of forming amixed-metal product by electrolysis wherein one metal of mixed-metalproduct is formed by electrorefining and another metal of the product isformed by electrowinning. For purposes of interpreting this disclosureand the claims that follow, the term “electrorefining” is defined torefer to a process in which a metal is transferred from an anode of anelectrolytic apparatus to a cathode. Accordingly, electrorefiningencompasses dissolution of a metal at an anode and deposition of thesame metal at a cathode. In contrast, the term “electrowinning” isdefined as a process wherein metal is transferred from electrolyte to acathode. Accordingly, an electrowinning process does not requiredissolution of a metal from an anodic material.

[0014] A process of the present invention is described with reference toFIG. 1. Specifically, FIG. 1 illustrates an exemplary electrolytic cell10 comprising a cathode 12 and anode 14 which are electrically connectedthrough a power source (not shown) to provide a potential difference 16(i.e., a voltage) between the anode and cathode. Electrolytic cell 10further comprises a vessel 18 which retains an electrolyte solution 20therein. Vessel 18 comprises a furnace 22 and a liner 24 on an interiorsurface of furnace 22. Liner 24 can comprise, for example, graphite.Furnace 22 is utilized to maintain elecrolytic solution 20 above amelting temperature of the solution, and further can be utilized tomaintain a substantially constant temperature during an electrolyticprocess of the present invention. Electrolytic solution 20 extendsbetween cathode 12 and anode 14, and accordingly completes an electricalcircuit comprising cathode 12 and anode 14.

[0015] A reactant material 26 is shown joined with anode 14. Reactantmaterial 26 can comprise a first metallic element. Although the shownembodiment has reactant material 26 provided as a discrete materialrelative to anode 14, it is to be understood that material 26 and anode14 can comprise a one-piece construction, with anode 14 having asubstantially homogenous composition of the first element. If thereactant material 26 is provided as a separate piece from the remainderof anode 14, reactant material 26 can be joined to the remainder ofanode 14 through a conductive interface, such as, for example, through aconductive epoxy, or a welded, brazed, or solid-diffused joint. Inalternative embodiments, the anode 14 can have a cupped shape, andmaterial 26 can be retained within the cupped shape. For instance, anode14 can be configured as a basket. In other embodiments, liner 24 can beutilized as the anode, and material 26 can be provided on the bottom ofvessel 18 and lying in electrical connection with liner 24. As long asmaterial 26 is in electrical connection with the remainder of an anodicmaterial, material 26 can be considered as being part of an anode duringan electrolytic operation. Accordingly, electrolytic operation willcomprise consumption of material from anodic component 26 andredeposition of the material onto cathode 12. In other words, theelectrolytic operation will comprise electrorefining of material fromanodic component 26.

[0016] In the shown embodiment, a product 28 is illustrated being formedaround a portion of cathode 12. Cathode 12 preferably comprises amaterial which is non-reactive with product 28, so that product 28 canbe readily removed from cathode 12 after an electrolytic process. Toreduce contamination in the cathode deposit, it can be preferred to usethe same or a similar material as the cathode material. In particularapplications, cathode 12 can comprise, for example, a titanium rod.

[0017] Although product 28 is shown formed on cathode 12 in theillustrated process, it is to be understood that the inventionencompasses other embodiments wherein material 28 is formed relative tocathode 12 and then shed from the cathode. In such embodiments, material28 can be collected on a shelf (not shown) provided beneath cathode 12,or in a basket (not shown) surrounding a portion of cathode 12.

[0018] Electrolytic solution 20 comprises an element different from theelement which is electrorefined from anode 26. The elementelectrorefined from anode 26 can be considered a first element, and thedifferent element in electrolytic solution 20 can be considered a secondelement. The second element can be provided as a compound withinelectrolytic solution 20, and in particular embodiments can be providedas a salt. The second element is transferred from solution 20 to product28, and accordingly is electrowon during the electrolytic operation ofapparatus 10. The first and second elements transferred to product 28are typically metals, and accordingly product 28 can be a mixed-metalproduct comprising a first metal formed by an electrorefining processand a second metal formed by an electrowinning process.

[0019] The first and second metals of product 28 may not be formedentirely by the eletrorefining and electrowinning processes,respectively. If anode 26 comprises a mixture of both elements and theelectrolytic process is operated at a cell voltage sufficiently largefor both metals to be anodically dissolved and cathodically deposited,an amount of the second element formed within product 28 will resultfrom an electrorefining process. Also, if there are contaminatescontaining the first element within electrolyte 20, an amount of thefirst element within product 28 will result from the electrowinningprocess. To account for such contributions of electrorefining andelectrowinning, product 28 can be described as being formed by primarilyelectrorefining of the first element from anode 26 and by primarilyelectrowinning of the second element from electrolyte 20. In suchdescription, the term “primarily” indicates that there may be someelectrowinning of the first element and some electrorefining of thesecond element.

[0020] Although product 28 is described as comprising as a mixture oftwo elements, it is to be understood that product 28 can also comprisemixtures of more than two elements. For example, a mixture of elementscan be provided in anodic component 26 so that more than one element iselectrorefined and formed in product 28 with the electrowon element fromelectrolyte 20. Alternatively, or additionally, more than one elementcan be provided within electrolyte 20 to be electrowon during theelectrorefining of one or more elements from anodic component 26. Themixed elements of product 28 will typically together define an alloycomposition.

[0021] Processing of the present invention can be utilized to formmaterials 28 comprising mixtures of numerous elements. For instance,product 28 can comprise, consist of, or consist essentially of, two ormore of tantalum, titanium, hafnium, zirconium and niobium.Alternatively, product 28 can comprise, consist of, or consistessentially of at least one of tantalum, titanium, hafnium, zirconiumand niobium in combination with at least one of vanadium, aluminum,chromium, and nickel. In exemplary applications, product 28 can comprisea mixture of tantalum and titanium; titanium and hafnium; titanium andzirconium; titanium and vanadium; titanium and aluminum; titanium andchromium; tantalum and zirconium; tantalum and chromium; or tantalum andnickel.

[0022] In particular applications, product 28 can consist of, or consistessentially of, mixtures of titanium and other materials selected fromthe group consisting of one or more of hafnium, zirconium, tantalum,vanadium, aluminum, chromium, nickel, and niobium. Such product cancomprise, for example, from about 5% titanium to about 95% titanium;from about 5% to about 25% titanium; from about 25% to about 50%titanium; from about 50% to about 75% titanium; or from about 75% toabout 95% titanium.

[0023] In other particular applications, product 28 can consist of, orconsist essentially of, mixtures of tantalum and other materialsselected from the group consisting of one or more of hafnium, zirconium,titanium, vanadium, aluminum, chromium, nickel, and niobium. Suchproduct can comprise, for example, from about 5% tantalum to about 95%tantalum; from about 5% to about 25% tantalum; from about 25% to about50% tantalum; from about 50% to about 75% tantalum; or from about 75% toabout 95% tantalum.

[0024] In yet other particular applications, product 28 can consist of,or consist essentially of, mixtures of hafnium and other materialsselected from the group consisting of one or more of tantalum,zirconium, titanium, vanadium, aluminum, chromium, nickel, and niobium.Such product can comprise, for example, from about 5% hafnium to about95% hafnium; from about 5% to about 25% hafnium; from about 25% to about50% hafnium; from about 50% to about 75% hafnium; or from about 75% toabout 95% hafnium.

[0025] In yet other particular applications, product 28 can consist of,or consist essentially of, mixtures of zirconium and other materialsselected from the group consisting of one or more of hafnium, tantalum,titanium, vanadium, aluminum, chromium, nickel, and niobium. Suchproduct can comprise, for example, from about 5% zirconium to about 95%zirconium; from about 5% to about 25% zirconium; from about 25% to about50% zirconium; from about 50% to about 75% zirconium; or from about 75%to about 95% zirconium.

[0026] In yet other particular applications, product 28 can consist of,or consist essentially of, mixtures of niobium and other materialsselected from the group consisting of one or more of hafnium, zirconium,titanium, vanadium, aluminum, chromium, nickel, and tantalum. Suchproduct can comprise, for example, from about 5% niobium to about 95%niobium; from about 5% to about 25% niobium; from about 25% to about 50%niobium; from about 50% to about 75% niobium; or from about 75% to about95% niobium.

[0027] In an exemplary embodiment of the present invention, product 28comprises a mixture of tantalum and titanium, wherein titanium is theelectrorefined element and tantalum is the electrowon element. In suchembodiment, titanium will be provided as an anodic material, and atantalum-containing compound will be provided within electrolyte 20. Thetantalum-containing compound can be a salt, such as, for example,K₂TaF₇. The titanium material of the anode can comprise relatively puretitanium, such as, for example, a material which is at least 99.9%titanium. Alternatively, the material can be a relativity impure form oftitanium, and the electrolytic process can be utilized to purify thetitanium during the electrorefining of the titanium and concomitantformation of titanium within product 28.

[0028] Electrolyte solution 20 is preferably maintained at a temperatureof from about 600° C. to about 850° C., and more preferably from about700° C. to about 750° C., during formation of a titanium/tantalumproduct 28.

[0029] A relative ratio of the first and second elements to one anotherwithin product 28 can be influenced and controlled by variousparameters. For example, the concentration ratio of the first element tothe second element in electrolyte 20 can alter the relative proportionsof the first and second elements in product 28. Also the temperature ofelectrolyte 20 can influence the kinetics of various half reactions inthe cell and thus alter the relative proportions of the first and secondelements in product 28. Another method to control the relative ratio ofthe first and second elements to one another within product 28 isdescribed below as a second embodiment with reference to FIG. 2.

[0030]FIG. 2 illustrates an apparatus 50 comprising a cathode 52 and apair of anodes 54 and 56. Apparatus 50 further includes a vessel 58comprising a furnace 80 and a liner 62; with an electrolyte solution 64shown contained within vessel 58. Vessel 58 can comprise a constructionidentical to that described above with reference to vessel 18 of FIG. 1.Cathode 52 can comprise a construction identical to that described abovewith reference to cathode 12, and anode 54 can comprise a constructionidentical to that described above with reference to anode 14. Thedifference between the apparatus 50 of FIG. 2 and the apparatus 10 ofFIG. 1 is that apparatus 50 comprises a second anode 56, in addition tothe first anode 54. Anode 54 is coupled to cathode 52 to a first voltage(or potential) 68, and anode 56 is coupled to cathode 52 to a secondvoltage 70.

[0031] In the shown construction, first anode 54 is coupled with areactant material 66 which is to be electrorefined during electrolyticoperation of apparatus 50. Anode 56, in contrast, is not coupled with areactant material. It is to be understood, however, that the inventionencompasses other embodiments (not shown) wherein anode 56 is coupledwith a reactant material. Preferably, in such constructions the reactantmaterial coupled with anode 56 will have a different concentration of anelement that is to be electrorefined than does the reactant material 66.

[0032] Electrolyte 64, like the electrolyte 20 of the FIG. 1 apparatus,comprises an element which is to be electrowon during electrolyticoperation of apparatus 50. In an exemplary application, this element canbe tantalum, and the reactant anodic material 66 can comprise titanium.

[0033] In operation, power is supplied to generate potentials 68 and 70,and such causes electrorefining of an element from anodic material 66and electrowinning of an element form electrolyte 64. The electrowon andelectrorefined elements together form a product 72. The relativeconcentration of the electrowon and electrorefined materials can beadjusted by adjusting voltage 68 relative to voltage 70.

[0034] In particular embodiments of the present invention, second anode56 comprises graphite, and the first anode comprises a titaniummaterial, such as, for example, a titanium reactant 66. (It is notedthat although anodic reactant 66 is shown separately coupled to anodiccomponent 54, the invention encompasses alternative embodiments (notshown) wherein anodic component 54 itself comprises the titaniummaterial, and wherein the separate anodic material 66 is not utilized).

[0035] Generally, voltage 68 and voltage 70 are determined by thedesired half reactions at each anode and at cathode. In an exemplarycase, the desired half reaction at anode 54 is Ti−2e=Ti²⁺; whereas atanode 56 a reaction of fluorine gas generation is desired: 2F⁻−2e=F₂. Atthe cathode, two reaction are desirable: Ti²⁺+2e=Ti and Ta⁵⁺+5e=Ta.Voltage 68 and voltage 70 should be large enough to ensure that thesereactions take place. The relative magnitude of voltage 68 to voltage 70can dictate the amount of titanium transferred to product 72.Specifically, if the magnitude of voltage 68 is reduced relative to themagnitude of voltage 70, less titanium will be transferred to product72. Accordingly, a relative concentration of tantalum in material 72 canbe decreased by decreasing the magnitude of voltage 68 relative to themagnitude of voltage 70. In particular applications, the magnitude ofvoltage 68 relative to voltage 70 will be fixed during formation ofproduct 72. In other applications, the magnitude of voltage 68 will bevaried relative to the magnitude of voltage 70 during product formation,and such can cause a relative concentration of tantalum and titanium tobe varied within product 72.

[0036] In particular embodiments, first anode 54 and second anode 56 canboth comprise titanium, but at different concentrations relative to oneanother. In such applications, the relative concentration of titanium inmaterial 72 can still be adjusted by adjusting the potential 68 relativeto the potential 70. Specifically, if anode 54 comprises a higherconcentration of titanium than anode 56, then a higher relativemagnitude of potential 68 to potential 70 will result in more titaniumbeing electrorefined in product 72 than would be electrorefined with alower relative magnitude of potential 68 to potential 70.

[0037] In still other particular embodiments of the present invention,anode 56 will not comprise an element which is to be electrorefined, butwill instead comprise, for example, carbon, and will therefore beutilized for electrowinning only. For instance, anode 56 canpredominantly comprise carbon (for example, graphite), consistessentially of carbon, or consist of carbon.

[0038] Although the embodiment of FIG. 2 is described as forming a mixedmetal product comprising two different elements, it is to be understoodthat the embodiment can be utilized for forming mixed metal productscomprising more than two elements. For instance, multiple elements canbe electrorefined and combined with an electrowon element to formproduct 72. Alternatively, multiple elements can be electrowon andcombined with an electrorefined element. In yet other alternativeembodiments, multiple materials can be electrorefined and combined withmultiple materials which are simultaneously electrowon to form theresultant product.

[0039] Once a mixed metal product is formed (either 28 of FIG. 1 or 72of FIG. 2, for example) the mixed metal product can be subjected tofurther processing to yield a material suitable for industrialapplications. For instance, the mixed metal product can be melted andcast into an ingot form. Since the mixed metal product is formed bycodeposition of two or more metals, it is essentially microscopicallyhomogeneous and the deposition process can be, in fact, an alloyingprocess. The melting point of the alloyed mixed metal product will bebetween the melting points of the constituent metal elements. For amixed titanium-tantalum product, this means that it will melt below2996° C., but above 1670° C. The actual melting temperature is dependenton the proportions of both elements. A lower melting temperature canmake a melting process much easier. Accordingly, a mixed metal productof this invention comprising a titanium/tantalum alloy can be a moresuitable feedstock for melting and forming tantalum-containing ingotsthan would be a material comprising pure tantalum or a material mixturecomprising pure tantalum and pure titanium in a non-alloyed state.

[0040] The relative amount of tantalum and titanium in product 28 (orproduct 72), and in melted ingots formed from the product, can beadjusted so that either titanium or tantalum is the predominantmaterial. Further product 28 or melted ingots can consist essentiallyof, or consist of, titanium and tantalum. Ingots can be subjected tometallurgical processing (such as, for example, hot forging, hot or coldrolling, extrusion and thermal treatments,) to adjust textures and/orgrain sizes within the materials of the ingots to desired parameters.Attention should be paid to the solubility of tantalum in titaniumduring metallurgical processing. The solubility of tantalum in titaniumat 600° C. is about 12%. It reduces during cooling, and is, for example,only about 7% at 400° C. Thus, tantalum-rich precipitates can formduring cooling from a melting temperature or another higher processingtemperature, when tantalum exceeds its solubility in titanium. In alloyswith a low tantalum content, this is not a problem. But for highertantalum content, say higher than 7%, the precipitation could beundesirable. A method of reducing precipitate formation is to rapidlyquench the titanium/tantalum mixed metal product so that the tantalum islocked within the titanium matrix before the tantalum has an opportunityto form precipitates. The temperature and rate of the quench procedureare preferably chosen such that there is effectively no tantalum-richprecipitate present within the titanium/tantalum material after it hasbeen quenched. A suitable fluid for quenching the titanium/tantalummaterial is a liquid, such as, for example, water or oil.

[0041] Another way to prevent or reduce precipitation is to apply powdermetallurgy to form parts. The mixed metal product 28 or 72 isessentially free of segregation. When pressed into shapes and sinteredat a suitable temperature, parts can be free of precipitates and free ofsegregation. Therefore, the mixed metal product 28 or 72 can beconsidered a better starting material for a powder process than would bea material having a higher amount of segregation between elementalconstituents of the material.

[0042] The discussion above is directed toward forming titanium/tantalummaterials predominately comprising titanium and having effectively notantalum-rich precipitates therein. Methodology of the present inventioncan also be utilized to form titanium materials having tantalum-richprecipitates therein. Such materials can be formed if a tantalumconcentration exceeds the solubility of tantalum in titanium. A suitablethermomechanical process including forging, and/or rolling, and/orextrusion, and heat treatment can be performed to control the size, theshape and the distribution of the tantalum-rich precipitates.

[0043] The thermo-mechanically processed material can then be shapedinto a form suitable for desired industrial applications. For instance,the material can be shaped into a PVD target, such as, for example, asputtering target.

[0044]FIGS. 3 and 4 illustrate exemplary embodiments of a PVD targetassembly. Specifically, FIGS. 3 and 4 illustrate an assembly 100comprising a sputtering target 102 bonded to a backing plate 104. Theshown construction is an ENDURA™ construction, but it is to beunderstood that the invention can be utilized for forming other PVDtarget constructions. Further, although the shown embodiment has asputtering target 102 bonded to a backing plate 104, it is to beunderstood that the invention also encompasses embodiments wherein themixed metal target is a monolithic target. In such embodiments, themixed metal can be formed into a target having a shape of apparatus 100,and accordingly wherein there is no backing plate 104. The mixed metalproduct can be formed into a target shape (such as, for example, theshape of target 102; or the shape of a monolithic target) byconventional metal-working methodology.

[0045] It can be advantageous to have a target 102 comprising a mixtureof tantalum and titanium. For instance, PVD targets are frequentlyutilized for sputter deposition of tantalum in forming semiconductorconstructions. Tantalum can be a desired barrier layer in constructionscomprising copper, in that tantalum can impede copper diffusion.However, tantalum is a relatively expensive material. Accordingly, itcan be desired to form targets wherein tantalum is diluted withinanother, less expensive, material; and then to sputter-deposittantalum-containing films from such targets.

[0046] It can be advantageous to utilize methodology of the presentinvention for forming products comprising mixtures of titanium andtantalum, in that it is typically difficult to mix tantalum andtitanium. Specifically, tantalum and titanium have significantlydifferent melting points from one another (1670° C. for titanium and2996° C. for tantalum) and significantly different densities (4.5grams/centimeter³ for titanium and 16 grams/centimeter³ for tantalum).Accordingly, segregation between titanium and tantalum frequentlyhappens during either melting or powder processing of titanium andtantalum in attempts to form mixtures of titanium and tantalum byconventional methodology. However, methodology of the present inventioncan form products comprising mixtures of titanium and tantalum withlittle or no segregation of titanium and tantalum within the products.

[0047] Exemplary targets comprising tantalum diluted in another materialare targets comprising a mixture of tantalum and titanium. In particularapplications, such targets can consist essentially of a mixture oftantalum and titanium, and in further applications such targets canconsist of a mixture of tantalum and titanium. Further, the targets canbe provided to a purity of 99.9% (3N) or higher (with the percentagebeing expressed in terms of weight percent; and with it being understoodthat percentage purities expressed herein are in terms of weight percentunless stated otherwise), with desired purities being 99.99%, 99.995%,99.999%, 99.9995%, or higher. Such purities can be obtained bymethodology of the present invention, in that electrorefining andelectrowinning methodology of the present invention can be utilized as apurification step, in addition to a step involved in formation of amixed metal product. Further, if it is desired to increase a purity of amixed metal product, such can be accomplished utilizing conventionalprocesses, such as, for example, e-beam melting.

[0048] In particular applications, a sputtering target of the presentinvention will comprise tantalum and titanium; consist of tantalum andtitanium, or consist essentially of tantalum and titanium. An exemplarytarget can comprise tantalum and titanium present to 99.9% purity orhigher, and will comprise a tantalum concentration of greater than 0%and less than 12%. The tantalum concentration can, for example, be fromabout 5% to about 12%; or from about 7% to about 12%. Alternatively, thetarget can comprise titanium to a concentration of at least about 50%,and can comprise tantalum to a concentration of less than or equal toabout 50%. In other alternative embodiments, the target can comprisemore than 50% tantalum, with the remainder of the target being titanium;with an exemplary PVD target consisting of tantalum and titanium, andhaving a tantalum concentration greater than or equal to about 5 weightpercent and less than or equal to about 95 weight percent.

1. A method for electrolytically forming a material which comprises at least two elements, the method comprising: providing an electrolytic cell comprising a cathode, an anode, and an electrolytic solution extending between the cathode and the anode; and electrolytically forming a metallic product with the electrolytic cell, the forming comprising primarily electrorefining of a first element of the at least two elements and primarily electrowinning of a second element of the at least two elements; the metallic product comprising the first and second elements.
 2. The method of claim 1 wherein the electrolytic cell comprises two anodes; one of the two anodes comprising the first element, and the other of the two anodes not comprising the first element.
 3. The method of claim 1 wherein the metallic product is formed on the cathode.
 4. The method of claim 1 wherein one of the first and second elements comprises titanium.
 5. The method of claim 1 wherein one of the first and second elements comprises titanium and the other of the first and second elements comprises hafnium.
 6. The method of claim 1 wherein one of the first and second elements comprises titanium and the other of the first and second elements comprises zirconium.
 7. The method of claim 1 wherein one of the first and second elements comprises titanium and the other of the first and second elements comprises vanadium.
 8. The method of claim 1 wherein one of the first and second elements comprises titanium and the other of the first and second elements comprises aluminum.
 9. The method of claim 1 wherein one of the first and second elements comprises titanium and the other of the first and second elements comprises chromium.
 10. The method of claim 1 wherein one of the first and second elements comprises tantalum and the other of the first and second elements comprises zirconium.
 11. The method of claim 1 wherein one of the first and second elements comprises tantalum and the other of the first and second elements comprises chromium.
 12. The method of claim 1 wherein one of the first and second elements comprises tantalum and the other of the first and second elements comprises nickel.
 13. The method of claim 1 wherein one of the first and second elements comprises tantalum.
 14. The method of claim 1 wherein one of the first and second elements comprises titanium and wherein the other of the first and second elements comprises tantalum.
 15. The method of claim 1 wherein the first element comprises titanium and wherein the second element comprises tantalum.
 16. The method of claim 1 wherein the first element comprises tantalum and wherein the second element comprises titanium.
 17. The method of claim 1 further comprising shaping the metallic product into a physical vapor deposition target.
 18. The method of claim 17 wherein the shaping comprises melting the metallic product into an ingot, and shaping the ingot into a physical vapor deposition target.
 19. A method for electrolytically forming a material which comprises at least two elements, the method comprising: providing an electrolytic cell comprising a cathode, at least two anodes, and an electrolytic solution extending between the cathode and the at least two anodes; the at least two anodes comprising first and second anodes having different concentrations of a first element relative to one another; the electrolytic solution comprising a compound which includes a second element; and electrolytically forming a metallic product with the electrolytic cell; the metallic product comprising a mixture of the first and second elements.
 20. The method of claim 19 wherein the first anode has a concentration of the first element which is greater than 0 weight percent; and wherein the second anode has a concentration of the first element which is about 0 weight percent.
 21. The method of claim 19 further comprising providing a first electrical potential difference between the first anode and the cathode and a second electrical potential difference between the second anode and the cathode; and wherein the second electrical potential difference is different than the first electrical potential difference.
 22. The method of claim 19 wherein the first element is a metallic element; wherein the first anode consists essentially of the first element; and wherein the second anode predominately comprises carbon.
 23. The method of claim 19 further comprising shaping the metallic product into a physical vapor deposition target.
 24. A method for electrolytically forming a material which comprises at least two elements, the method comprising: providing an electrolytic cell comprising a cathode, at least two anodes, and an electrolytic solution extending between the cathode and the at least two anodes; the electrolytic solution comprising a compound which includes a second element; and electrolytically forming a metallic product with the electrolytic cell; the metallic product comprising a mixture of the first and second elements; one of the at least two anodes being operated at a different voltage than an other of the at least two anodes during the electrolytically forming of the metallic product.
 25. The method of claim 24 further comprising shaping the metallic product into a physical vapor deposition target.
 26. A method for electrolytically forming a product which comprises a mixture of tantalum and titanium, the method comprising: providing an electrolytic cell comprising a cathode, an anode, and an electrolytic solution extending between the cathode and the anode; the anode comprising titanium and the electrolytic solution comprising a tantalum-containing compound; and electrolytically forming a metallic product with the electrolytic cell, the metallic product comprising a mixture of titanium from the anode and tantalum from the tantalum-containing compound.
 27. The method of claim 26 wherein the tantalum-containing compound is K₂TaF₇.
 28. The method of claim 26 wherein the electrolytic solution is maintained at a temperature of from about 700° C. to about 850° C. during the electrolytically forming of the metallic product.
 29. The method of claim 26 wherein the electrolytic solution is maintained at a temperature of from about 700° C. to about 750° C. during the electrolytically forming of the metallic product.
 30. The method of claim 26 further comprising shaping the metallic product into a physical vapor deposition target.
 31. The method of claim 26 further comprising pressing and sintering the metallic product.
 32. The method of claim 26 further comprising subjecting the metallic product to forces to reduce an average grain size present within the metallic product.
 33. A material which comprises a mixture of tantalum and titanium; and which is at least 99.9 weight percent tantalum and titanium.
 34. The material of claim 33 comprising at least about 50 weight percent titanium.
 35. The material of claim 33 comprising greater than 0 weight percent tantalum and less than or equal to about 12 weight percent tantalum.
 36. The material of claim 33 comprising greater than or equal t o about 7 weight percent tantalum and less than or equal to about 12 weight percent tantalum.
 37. The material of claim 33 being in the shape of a PVD target.
 38. A material which consists essentially of a mixture of tantalum and titanium.
 39. The material of claim 38 being in the shape of a PVD target.
 40. The material of claim 38 comprising more titanium than tantalum.
 41. The material of claim 38 comprising more tantalum than titanium.
 42. A material which consists essentially of: at least one first element selected from the group consisting of titanium, tantalum, zirconium, hafnium, and niobium; at least one second element selected from the group consisting of titanium, tantalum, zirconium, hafnium, niobium, vanadium, aluminum, chromium and nickel; and wherein the at least one first element is different from the at least one second element.
 43. The material of claim 42 wherein the first and second elements together define an alloy within the material.
 44. The material of claim 42 comprising tantalum to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 95 weight percent.
 45. The material of claim 42 comprising tantalum to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 25 weight percent.
 46. The material of claim 42 comprising tantalum to a concentration of greater than or equal to about 25 weight percent and less than or equal to about 50 weight percent.
 47. The material of claim 42 comprising tantalum to a concentration of greater than or equal to about 50 weight percent and less than or equal to about 75 weight percent.
 48. The material of claim 42 comprising tantalum to a concentration of greater than or equal to about 75 weight percent and less than or equal to about 95 weight percent.
 49. The material of claim 42 comprising titanium to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 95 weight percent.
 50. The material of claim 42 comprising titanium to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 25 weight percent.
 51. The material of claim 42 comprising titanium to a concentration of greater than or equal to about 25 weight percent and less than or equal to about 50 weight percent.
 52. The material of claim 42 comprising titanium to a concentration of greater than or equal to about 50 weight percent and less than or equal to about 75 weight percent.
 53. The material of claim 42 comprising titanium to a concentration of greater than or equal to about 75 weight percent and less than or equal to about 95 weight percent.
 54. The material of claim 42 comprising hafnium to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 95 weight percent.
 55. The material of claim 42 comprising hafnium to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 25 weight percent.
 56. The material of claim 42 comprising hafnium to a concentration of greater than or equal to about 25 weight percent and less than or equal to about 50 weight percent.
 57. The material of claim 42 comprising hafnium to a concentration of greater than or equal to about 50 weight percent and less than or equal to about 75 weight percent.
 58. The material of claim 42 comprising hafnium to a concentration of greater than or equal to about 75 weight percent and less than or equal to about 95 weight percent.
 59. The material of claim 42 comprising niobium to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 95 weight percent.
 60. The material of claim 42 comprising niobium to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 25 weight percent.
 61. The material of claim 42 comprising niobium to a concentration of greater than or equal to about 25 weight percent and less than or equal to about 50 weight percent.
 62. The material of claim 42 comprising niobium to a concentration of greater than or equal to about 50 weight percent and less than or equal to about 75 weight percent.
 63. The material of claim 42 comprising niobium to a concentration of greater than or equal to about 75 weight percent and less than or equal to about 95 weight percent.
 64. The material of claim 42 comprising zirconium to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 95 weight percent.
 65. The material of claim 42 comprising zirconium to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 25 weight percent.
 66. The material of claim 42 comprising zirconium to a concentration of greater than or equal to about 25 weight percent and less than or equal to about 50 weight percent.
 67. The material of claim 42 comprising zirconium to a concentration of greater than or equal to about 50 weight percent and less than or equal to about 75 weight percent.
 68. The material of claim 42 comprising zirconium to a concentration of greater than or equal to about 75 weight percent and less than or equal to about 95 weight percent.
 69. The material of claim 42 being in the shape of a PVD target.
 70. A PVD target comprising tantalum to a concentration of greater than or equal to about 5 weight percent and less than or equal to about 95 weight percent.
 71. The PVD target of claim 70 comprising the tantalum to a concentration of less than or equal to about 50 weight percent.
 72. The PVD target of claim 70 consisting essentially of tantalum and titanium. 